The present paper outlines the characterization, electrokinetic behaviour, and flotation response of rejected coking coal fines with 32.5% ash generated in a coal washery in Eastern India. The response methodology and central composite rotatable design (RSM-CCRD) were used for the process modelling and optimization of the flotation process using diesel, methyl isobutyl carbinol (MIBC), and sodium hexametaphosphate as a collector, frother, and depressant to maximize ash reduction, yield, and combustible recovery. At optimum condition, a 9.7% clean ash coal was achieved with a 63% yield at collector, frother, and depressant dosages of 0.78, 0.31, and 0.80 kg/ton, respectively. The model prediction and experimental data corroborated sufficiently. Subsequently, within 1 year, the fines oxidized and did not float with the collector. Fourier-transform infrared spectroscopy (FTIR) confirmed surface oxidation on oxidized coal. The oxidized coal responded favourably to acid oil, a vegetable oil refinery waste. With acid oil as a collector, the oxidized coal can upgrade to 12% clean ash coal with a 60% yield; the combustible recovered is 80%. The work indicates successful upgradation of fresh and oxidized coal using the froth flotation process.